2-butyl-2-ethylpropane-1,3-diol

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: With 4-nitrobenzylphosphonic acid and 2-butyl-2-ethyl-1,3-propanediol, the same procedure as in Reference Example 11 was followed, to yield 5-butyl-5-ethyl-2-(4-nitrobenzyl)- 1,3,2-dioxaphosphorinane-2-oxide, which was then recrystallized from ethanol-hexane to yield colorless prisms having a melting point of 111° to 112° C.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 15 parts of 1-amino-2-methoxy-4-hydroxyanthraquinone, 50 parts of 2-ethyl-2-butyl-1,3-propanediol, 2.5 parts of a polyethylene oxide of average moleclar weight 200 and 1.5 parts of potassium hydroxide are heated for 3.5 hours at 160°C under nitrogen. After working up, 13.5 parts of 1-amino-2-(2'-ethyl-2'-butyl-3'-hydroxypropanoxy)-4-hydroxyanthraquinone are obtained.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 15 parts of 1-amino-2-methoxy-4-hydroxyanthraquinone, 50 parts of 2-ethyl-2-butyl-1,3-propanediol, 2.5 parts of a polyethylene oxide of average moleclar weight 200 and 1.5 parts of potassium hydroxide are heated for 3.5 hours at 160°C under nitrogen. After working up, 13.5 parts of 1-amino-2-(2'-ethyl-2'-butyl-3'-hydroxypropanoxy)-4-hydroxyanthraquinone are obtained.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Nitrobenzylphosphonic acid and 2-butyl-2-ethyl-1,3-propanediol were treated in the same manner as in Reference Example 20 to yield 5-butyl-5-ethyl-2-(4-nitrobenzyl)-1,3,2-dioxaphosphorinan-2-oxide, which was then recrystallized from ethanol-hexane to yield colorless prisms having a melting point of 111°-112° C.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A process for producing 2-butyl-2-ethyl-1,3-propanediol, comprising feeding a hydroxide compound into a reaction mixture containing 2-ethylhexanal and formaldehyde wherein said hydroxide compound is fed into the reaction mixture continuously and incrementally to produce 2-butyl-2-ethyl-1,3-propanediol such that the reaction mixture is maintained in two phases, an organic phase and an aqueous phase throughout the entire production process.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: BEPD was prepared by a semi-batch process out of 2-ethylhexanal (2-EH), having a purity of over 90 weight-%, and formaline. The concentration of the formaline aqueous solution was 37 weight-% HCHO and it contained 10 weight-% CH3OH. First, 1207 g (9.225 moles) of 2-EH and 1911 g (23.546 moles) of HCHO were fed into the reactor to make up the reaction mixture, after which 927 g (11.125 moles) in total of sodium hydroxide was fed into the reaction mixture. The concentration of the sodium hydroxide aqueous solution was 48 weight-%, and it was fed for 6 hours at three input rates, namely 93 g/h (1.1161 moles per hour) during the first hour of the reaction (beginning at time T1), 135 g/h of NaOH (1.6201 moles/h; beginning at time T2) during the following two hours and, finally, 188 g/h (2.2562 moles/h; beginning at time T3) during the third to the 6th hour.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The molar ratio of the 2-ethyl hexanal to the formaldehyde, used as the initial materials of the reaction, should be within the range 1:2 to 1:4, preferably within the range 1:2.5 to 1:3.5. To the mixture is added a neutral or cationic phase transfer catalyst, such as neutral polyethylene glycol (e.g. PEG 400) or a cationic tetrabutylammoniumhydrogen sulfate (TBAHSO4) or tricaprylmethylammonium chloride (Aliquat 336). These are added in an amount of 1-50% by weight, preferably 5-30% by weight, of the mass of the formalin solution or, if solid paraformaldehyde is used, in an amount of 1-20% by weight, preferably 3-10% by weight, of the mass of the aqueous solution and solid paraformaidehyde, or in an amount of 1-50% by weight, preferably 5-15% by weight, of the amount of 2-ethyl hexanal. The mixture of the initial materials is heated to 30°-100° C., preferably to 50°-80° C., and most preferably to 60°-80° C., and an aqueous solution of the alkali metal hydroxide or earth alkali metal hydroxide is added to the mixture, drop by drop, in the course of up to 5 h, preferably 1-3 h, and the reaction is continued at the said temperature for up to 3 h, preferably 15 min-2 h, most preferably 15 min-1 h 15 min. The alkali metal hydroxide or earth alkali metal hydroxide is used in a molar amount 1:1 to 2:1, preferably in a molar amount of 1.25:1 to 1.75:1 to that of 2:1-ethyl hexanal. After this reaction step the mixture is neutralized with an organic acid or a mineral acid, preferably for example sulfuric acid, and the phases are separated from each other, preferably while they are hot. The organic phase is washed with water once or several times, preferably 1-2 times, by using for the wash an amount of water at minimum 50% of the mass of the organic phase. The phases are separated and the organic phases are combined and vacuum distilled. The boiling point of the final product is 130°-132° C./9 mmHg. The yield obtained for 2-n-butyl-2-ethyl-1,3-propane diol was up to more than 92%, depending on the reaction conditions and the molar proportions. To the mixture is added a neutral or cationic phase transfer catalyst is heated to 30°-100° C., preferably to 50°-80° C. preferably 1-3 h up to 3 h preferably 15 min-2 h, most preferably 15 min-1 h 15 min After this reaction step the mixture The organic phase is washed with water once wash an amount of water at minimum 50% of the mass of the organic phase The phases are separated vacuum distilled is 130°-132° C.

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The molar ratio of the 2-ethyl hexanal to the formaldehyde, used as the initial materials of the reaction, should be within the range 1:2 to 1:4, preferably within the range 1:2.5 to 1:3.5. To the mixture is added a neutral or cationic phase transfer catalyst, such as neutral polyethylene glycol (e.g. PEG 400) or a cationic tetrabutylammoniumhydrogen sulfate (TBAHSO4) or tricaprylmethylammonium chloride (Aliquat 336). These are added in an amount of 1-50% by weight, preferably 5-30% by weight, of the mass of the formalin solution or, if solid paraformaldehyde is used, in an amount of 1-20% by weight, preferably 3-10% by weight, of the mass of the aqueous solution and solid paraformaidehyde, or in an amount of 1-50% by weight, preferably 5-15% by weight, of the amount of 2-ethyl hexanal. The mixture of the initial materials is heated to 30°-100° C., preferably to 50°-80° C., and most preferably to 60°-80° C., and an aqueous solution of the alkali metal hydroxide or earth alkali metal hydroxide is added to the mixture, drop by drop, in the course of up to 5 h, preferably 1-3 h, and the reaction is continued at the said temperature for up to 3 h, preferably 15 min-2 h, most preferably 15 min-1 h 15 min. The alkali metal hydroxide or earth alkali metal hydroxide is used in a molar amount 1:1 to 2:1, preferably in a molar amount of 1.25:1 to 1.75:1 to that of 2:1-ethyl hexanal. After this reaction step the mixture is neutralized with an organic acid or a mineral acid, preferably for example sulfuric acid, and the phases are separated from each other, preferably while they are hot. The organic phase is washed with water once or several times, preferably 1-2 times, by using for the wash an amount of water at minimum 50% of the mass of the organic phase. The phases are separated and the organic phases are combined and vacuum distilled. The boiling point of the final product is 130°-132° C./9 mmHg. The yield obtained for 2-n-butyl-2-ethyl-1,3-propane diol was up to more than 92%, depending on the reaction conditions and the molar proportions. To the mixture is added a neutral or cationic phase transfer catalyst is heated to 30°-100° C., preferably to 50°-80° C. preferably 1-3 h up to 3 h preferably 15 min-2 h, most preferably 15 min-1 h 15 min After this reaction step the mixture The organic phase is washed with water once wash an amount of water at minimum 50% of the mass of the organic phase The phases are separated vacuum distilled is 130°-132° C.